######################################## # # # CIF generated by the Xtal System # # # ######################################## data_global _audit_creation_method Xtal3.6 _audit_creation_date 03-03-31 _audit_update_record ? #============================================================================== # (Publishing Staff Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================================= # 1. SUBMISSION DETAILS #---------------------- _publ_contact_author_name 'Skelton, B. W.' _publ_contact_author_address ; Department of Chemistry University of Western Australia 35 Stirling Highway Crawley Western Australia 6009 Australia ; _publ_contact_author_email bws@crystal.uwa.edu.au _publ_contact_author_fax (+61)_08_9380_1118 _publ_contact_author_phone (+61)_08-9380_3481 _publ_contact_letter ; ? #<< contact letter ; _publ_requested_journal ? _publ_requested_category ? _publ_section_title ; ? #<< paper title text ; _publ_section_title_footnote ; ? #<< paper footnote text ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Skelton, Brian W.' . ; Department of Chemistry, University of Western Australia, 35 Stirling Highway, Crawley, WA 6009, Australia. ; _publ_section_synopsis ; ? #<< synopsis if FI,CI,CM,CO papers ; _publ_section_abstract ; ? #<< abstract text ; _publ_section_comment ; ? #<< scientific commentary text ; _publ_section_exptl_prep ; ? #<< material & crystal preparation text ; _publ_section_exptl_refinement ; ? #<< crystallographic methods used ; _publ_section_acknowledgements ; ? #<< acknowledgements text ; _publ_section_references ; Sheldrick, G M. (1996). SADABS. Pogram for Empirical Absorption Correction of Area Detector Data. University of Gottingen, Germany. Siemens (1995). SMART and SAINT. Area-Detector Control and Integration Software. Siemens Analytical X-ray Systems Inc., Madison, Wisconsin, USA. Hall, S.R., King, G.S.D., and Stewart., J.M. (1995). The Xtal 3.5 User's Manual. University of Western Australia, Lamb: Perth. ; _publ_section_figure_captions ; ? #<< figure captions ; #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_bim10 # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C12 H26 Cu1 F12 N6 O3 P2' _chemical_formula_moiety ? _chemical_formula_weight 655.85 _chemical_melting_point ? _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P_21_21_21 _symmetry_space_group_name_Hall p_2ac_2ab loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,-y,1/2+z 1/2+x,1/2-y,-z -x,1/2+y,1/2-z _cell_length_a 9.375(3) _cell_length_b 14.682(4) _cell_length_c 17.196(5) _cell_angle_alpha 90.00000 _cell_angle_beta 90.00000 _cell_angle_gamma 90.00000 _cell_volume 2366.9(12) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.84 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 6114 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 34.12 _cell_measurement_temperature 153 _exptl_absorpt_coefficient_mu 1.181 _exptl_crystal_description prism _exptl_crystal_size_max .35 _exptl_crystal_size_mid .23 _exptl_crystal_size_min .16 _exptl_crystal_size_rad ? _exptl_crystal_colour blue _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .69 _exptl_absorpt_correction_T_max 1 _diffrn_reflns_number 10327 _reflns_number_total 5713 _reflns_Friedel_coverage .96 _reflns_number_gt 4980 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 35.11 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .042 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 27 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .037 _refine_ls_wR_factor_ref .048 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_number_reflns 4921 _refine_ls_number_parameters 430 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment refall _refine_ls_shift/su_max .011 _refine_diff_density_min -.635 _refine_diff_density_max .985 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack xabs refined' _refine_ls_abs_structure_Flack -.009(10) # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 48 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 104 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cu ? 0 4 .263 1.266 'Int Tables Vol IV Tables 2.2B and 2.3.1' F ? 0 48 .014 .01 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 24 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 12 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' P ? 0 8 .09 .095 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cu .32266(4) .39745(2) .69630(2) .01357(12) Uani ? ? 1.00000 ? ? O1 .2405(2) .39036(14) .80129(12) .0164(8) Uani ? ? 1.00000 ? ? O2 .2954(2) .38012(16) .92760(12) .0195(9) Uani ? ? 1.00000 ? ? O3 .6091(3) .1905(2) .9678(2) .0320(14) Uani ? ? 1.00000 ? ? N1 .2953(3) .25526(18) .65539(16) .0210(11) Uani ? ? 1.00000 ? ? N2 .1308(3) .41849(19) .64386(16) .0203(11) Uani ? ? 1.00000 ? ? N3 .4033(3) .41487(17) .58704(15) .0185(10) Uani ? ? 1.00000 ? ? N4 .5070(3) .40966(19) .75529(14) .0173(10) Uani ? ? 1.00000 ? ? N5 .7898(3) .3064(2) .89773(17) .0225(12) Uani ? ? 1.00000 ? ? N6 .9688(3) .3814(3) .85188(17) .0272(13) Uani ? ? 1.00000 ? ? C1 .1381(4) .2477(2) .6566(2) .0263(15) Uani ? ? 1.00000 ? ? C2 .0675(4) .3303(3) .6178(2) .0266(15) Uani ? ? 1.00000 ? ? C3 .1624(4) .4821(2) .57850(19) .0233(13) Uani ? ? 1.00000 ? ? C4 .2890(4) .4466(2) .53299(18) .0235(13) Uani ? ? 1.00000 ? ? C5 .4674(4) .3267(2) .5640(2) .0245(14) Uani ? ? 1.00000 ? ? C6 .3632(4) .2477(2) .5777(2) .0251(14) Uani ? ? 1.00000 ? ? C7 .3295(3) .38345(16) .85847(15) .0142(10) Uani ? ? 1.00000 ? ? C8 .4868(3) .3739(2) .83502(15) .0141(10) Uani ? ? 1.00000 ? ? C9 .5871(3) .4176(2) .89489(17) .0188(12) Uani ? ? 1.00000 ? ? C10 .7406(3) .3931(2) .88129(16) .0180(11) Uani ? ? 1.00000 ? ? C11 .8534(3) .4397(3) .8524(2) .0241(14) Uani ? ? 1.00000 ? ? C12 .9274(4) .3014(3) .8794(2) .0279(15) Uani ? ? 1.00000 ? ? P1 .27004(8) .65016(5) .80698(5) .0182(3) Uani ? ? 1.00000 ? ? F11 .2921(3) .59256(19) .72885(14) .0390(13) Uani ? ? 1.00000 ? ? F12 .1622(3) .7171(2) .76375(16) .0399(13) Uani ? ? 1.00000 ? ? F13 .2505(3) .70776(16) .88625(13) .0313(11) Uani ? ? 1.00000 ? ? F14 .3803(3) .58395(16) .85112(16) .0322(11) Uani ? ? 1.00000 ? ? F15 .4010(3) .71536(16) .78255(14) .0298(10) Uani ? ? 1.00000 ? ? F16 .1409(2) .58578(16) .83243(16) .0327(11) Uani ? ? 1.00000 ? ? P2 .75516(9) .57804(6) .64940(5) .0208(3) Uani ? ? 1.00000 ? ? F21 .9099(3) .5753(2) .6885(2) .0458(14) Uani ? ? 1.00000 ? ? F22 .7574(4) .68615(17) .6485(2) .0484(16) Uani ? ? 1.00000 ? ? F23 .5971(3) .5781(2) .6126(2) .0497(16) Uani ? ? 1.00000 ? ? F24 .7482(3) .46856(15) .65232(15) .0364(12) Uani ? ? 1.00000 ? ? F25 .8234(4) .5736(3) .56561(16) .0588(19) Uani ? ? 1.00000 ? ? F26 .6850(3) .58115(17) .73502(15) .0354(11) Uani ? ? 1.00000 ? ? H3aO .560(8) .158(5) .947(4) .05(2) Uiso ? ? 1.00000 ? ? H3bO .648(8) .167(5) 1.001(4) .06(2) Uiso ? ? 1.00000 ? ? H1 .330(5) .222(3) .685(3) .021(11) Uiso ? ? 1.00000 ? ? H2 .070(6) .448(4) .673(3) .033(14) Uiso ? ? 1.00000 ? ? H3 .467(5) .453(3) .588(3) .019(11) Uiso ? ? 1.00000 ? ? H4aN .573(5) .383(3) .735(3) .018(10) Uiso ? ? 1.00000 ? ? H4bN .525(7) .466(5) .757(3) .043(16) Uiso ? ? 1.00000 ? ? H5 .752(8) .266(5) .919(4) .050(18) Uiso ? ? 1.00000 ? ? H6 1.065(7) .385(4) .838(3) .040(15) Uiso ? ? 1.00000 ? ? H1a .119(5) .245(3) .707(3) .016(10) Uiso ? ? 1.00000 ? ? H1b .107(6) .193(4) .630(3) .031(13) Uiso ? ? 1.00000 ? ? H2a .076(5) .327(3) .562(3) .022(11) Uiso ? ? 1.00000 ? ? H2b -.037(6) .334(4) .629(3) .027(12) Uiso ? ? 1.00000 ? ? H3a .178(6) .539(4) .600(3) .035(14) Uiso ? ? 1.00000 ? ? H3b .081(5) .487(3) .547(2) .014(10) Uiso ? ? 1.00000 ? ? H4a .264(6) .401(4) .502(3) .035(13) Uiso ? ? 1.00000 ? ? H4b .321(6) .494(3) .498(3) .026(12) Uiso ? ? 1.00000 ? ? H5a .547(5) .317(3) .590(2) .009(9) Uiso ? ? 1.00000 ? ? H5b .492(6) .330(4) .512(3) .028(12) Uiso ? ? 1.00000 ? ? H6a .299(6) .247(3) .537(3) .023(12) Uiso ? ? 1.00000 ? ? H6b .415(6) .189(4) .574(3) .032(13) Uiso ? ? 1.00000 ? ? H8 .498(6) .315(4) .833(3) .031(13) Uiso ? ? 1.00000 ? ? H9a .554(5) .398(3) .943(3) .016(10) Uiso ? ? 1.00000 ? ? H9b .590(7) .486(4) .895(3) .040(15) Uiso ? ? 1.00000 ? ? H11 .853(6) .504(3) .835(3) .029(13) Uiso ? ? 1.00000 ? ? H12 .992(6) .252(4) .886(3) .033(14) Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cu .01223(12) .01486(12) .01361(11) -.00018(11) -.00142(11) -.00001(11) O1 .0106(7) .0208(8) .0177(8) -.0007(6) -.0004(7) .0003(8) O2 .0182(10) .0236(10) .0168(8) -.0001(7) .0033(7) -.0010(7) O3 .0294(14) .0305(13) .0363(14) -.0038(11) -.0102(11) .0100(11) N1 .0265(13) .0159(10) .0206(11) .0007(9) -.0051(9) .0019(9) N2 .0185(10) .0207(11) .0217(11) .0014(9) -.0055(9) .0012(9) N3 .0221(11) .0167(10) .0167(9) -.0014(8) -.0004(8) .0014(8) N4 .0128(9) .0233(12) .0158(9) -.0030(8) .0018(7) .0003(8) N5 .0148(11) .0273(13) .0254(12) .0028(9) -.0024(9) .0014(10) N6 .0114(10) .0474(19) .0228(11) -.0012(11) -.0008(9) -.0006(12) C1 .0257(15) .0213(13) .0319(17) -.0077(11) -.0071(12) .0059(12) C2 .0231(15) .0264(15) .0304(15) -.0054(12) -.0120(12) .0028(12) C3 .0284(15) .0178(12) .0237(13) .0047(11) -.0068(11) .0024(10) C4 .0345(17) .0192(12) .0168(11) .0041(11) -.0052(11) .0023(10) C5 .0297(16) .0233(13) .0204(12) .0075(12) .0038(11) .0010(11) C6 .0380(18) .0162(12) .0209(13) .0037(11) -.0022(11) -.0014(10) C7 .0111(9) .0135(10) .0179(10) .0008(8) .0006(8) -.0019(8) C8 .0100(10) .0181(11) .0142(10) .0006(8) .0008(8) -.0008(8) C9 .0122(10) .0266(14) .0177(11) .0015(9) -.0021(8) -.0050(10) C10 .0117(10) .0250(12) .0172(10) .0007(10) -.0018(8) -.0013(10) C11 .0156(12) .0351(16) .0217(12) -.0041(11) -.0015(10) .0052(12) C12 .0130(12) .0406(19) .0300(15) .0065(12) -.0016(11) -.0057(14) P1 .0183(3) .0158(3) .0206(3) .0004(2) -.0010(3) .0008(3) F11 .0490(15) .0365(12) .0315(11) -.0077(11) .0037(10) -.0138(10) F12 .0362(13) .0417(13) .0419(13) .0098(11) -.0089(11) .0168(11) F13 .0429(13) .0262(10) .0249(9) -.0025(10) .0092(9) -.0041(8) F14 .0255(10) .0260(10) .0452(13) .0065(8) -.0053(10) .0089(9) F15 .0322(11) .0248(10) .0325(10) -.0086(8) .0069(9) .0014(8) F16 .0230(9) .0275(11) .0475(13) -.0079(8) .0016(9) .0022(9) P2 .0191(3) .0193(3) .0241(3) -.0029(3) .0012(3) .0033(3) F21 .0213(10) .0568(16) .0593(17) .0008(11) -.0080(12) -.0038(15) F22 .0560(18) .0207(10) .069(2) -.0086(11) -.0051(17) .0122(12) F23 .0353(14) .0443(15) .069(2) -.0012(12) -.0256(14) -.0003(14) F24 .0489(15) .0184(9) .0420(13) .0021(10) .0138(12) -.0038(9) F25 .071(2) .076(2) .0294(12) -.014(2) .0194(14) .0096(14) F26 .0428(13) .0293(10) .0342(11) .0009(10) .0133(10) -.0082(9) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Cu O1 . . 1.965(2) ? Cu N1 . . 2.218(3) ? Cu N2 . . 2.035(3) ? Cu N3 . . 2.041(3) ? Cu N4 . . 2.012(3) ? Cu F11 . . 2.933(3) ? O1 C7 . . 1.293(3) ? O2 C7 . . 1.232(3) ? O3 H3aO . . .76(8) ? O3 H3bO . . .76(7) ? N1 C1 . . 1.479(5) ? N1 C6 . . 1.484(4) ? N1 H1 . . .77(5) ? N2 C2 . . 1.494(5) ? N2 C3 . . 1.491(4) ? N2 H2 . . .87(6) ? N3 C4 . . 1.493(4) ? N3 C5 . . 1.481(4) ? N3 H3 . . .83(5) ? N4 C8 . . 1.480(4) ? N4 H4aN . . .81(5) ? N4 H4bN . . .84(7) ? N5 C10 . . 1.384(5) ? N5 C12 . . 1.330(4) ? N5 H5 . . .78(7) ? N6 C11 . . 1.378(5) ? N6 C12 . . 1.325(6) ? N6 H6 . . .94(6) ? C1 C2 . . 1.534(5) ? C1 H1a . . .89(5) ? C1 H1b . . .98(6) ? C2 H2a . . .97(5) ? C2 H2b . . 1.00(5) ? C3 C4 . . 1.515(5) ? C3 H3a . . .93(6) ? C3 H3b . . .94(5) ? C4 H4a . . .88(6) ? C4 H4b . . .96(5) ? C5 C6 . . 1.533(5) ? C5 H5a . . .88(4) ? C5 H5b . . .93(5) ? C6 H6a . . .92(5) ? C6 H6b . . .99(6) ? C7 C8 . . 1.535(4) ? C8 C9 . . 1.535(4) ? C8 H8 . . .87(6) ? C9 C10 . . 1.502(4) ? C9 H9a . . .94(5) ? C9 H9b . . 1.00(6) ? C10 C11 . . 1.354(4) ? C11 H11 . . .99(5) ? C12 H12 . . .95(6) ? P1 F11 . . 1.601(3) ? P1 F12 . . 1.594(3) ? P1 F13 . . 1.615(2) ? P1 F14 . . 1.609(3) ? P1 F15 . . 1.613(3) ? P1 F16 . . 1.597(3) ? P2 F21 . . 1.599(3) ? P2 F22 . . 1.588(3) ? P2 F23 . . 1.611(3) ? P2 F24 . . 1.610(2) ? P2 F25 . . 1.578(3) ? P2 F26 . . 1.613(3) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published O1 Cu N1 . . . 101.32(10) ? O1 Cu N2 . . . 93.95(10) ? O1 Cu N3 . . . 175.67(10) ? O1 Cu N4 . . . 82.99(9) ? O1 Cu F11 . . . 80.68(8) ? N1 Cu N2 . . . 84.28(11) ? N1 Cu N3 . . . 82.46(10) ? N1 Cu N4 . . . 110.06(11) ? N1 Cu F11 . . . 165.62(9) ? N2 Cu N3 . . . 84.29(11) ? N2 Cu N4 . . . 165.65(11) ? N2 Cu F11 . . . 81.37(10) ? N3 Cu N4 . . . 97.74(11) ? N3 Cu F11 . . . 95.13(9) ? N4 Cu F11 . . . 84.30(10) ? Cu O1 C7 . . . 116.74(17) ? H3aO O3 H3bO . . . 112(8) ? Cu N1 C1 . . . 100.5(2) ? Cu N1 C6 . . . 107.8(2) ? Cu N1 H1 . . . 110(4) ? C1 N1 C6 . . . 115.7(3) ? C1 N1 H1 . . . 112(4) ? C6 N1 H1 . . . 111(4) ? Cu N2 C2 . . . 110.6(2) ? Cu N2 C3 . . . 104.7(2) ? Cu N2 H2 . . . 113(4) ? C2 N2 C3 . . . 113.3(3) ? C2 N2 H2 . . . 110(4) ? C3 N2 H2 . . . 104(4) ? Cu N3 C4 . . . 110.3(2) ? Cu N3 C5 . . . 106.7(2) ? Cu N3 H3 . . . 109(3) ? C4 N3 C5 . . . 113.4(2) ? C4 N3 H3 . . . 109(3) ? C5 N3 H3 . . . 108(3) ? Cu N4 C8 . . . 108.99(17) ? Cu N4 H4aN . . . 113(3) ? Cu N4 H4bN . . . 106(4) ? C8 N4 H4aN . . . 109(3) ? C8 N4 H4bN . . . 110(4) ? H4aN N4 H4bN . . . 109(6) ? C10 N5 C12 . . . 109.0(3) ? C10 N5 H5 . . . 130(5) ? C12 N5 H5 . . . 121(5) ? C11 N6 C12 . . . 108.6(3) ? C11 N6 H6 . . . 136(4) ? C12 N6 H6 . . . 115(4) ? N1 C1 C2 . . . 111.4(3) ? N1 C1 H1a . . . 103(3) ? N1 C1 H1b . . . 111(3) ? C2 C1 H1a . . . 112(3) ? C2 C1 H1b . . . 109(3) ? H1a C1 H1b . . . 111(4) ? N2 C2 C1 . . . 112.5(3) ? N2 C2 H2a . . . 108(3) ? N2 C2 H2b . . . 106(3) ? C1 C2 H2a . . . 111(3) ? C1 C2 H2b . . . 113(3) ? H2a C2 H2b . . . 106(4) ? N2 C3 C4 . . . 109.2(3) ? N2 C3 H3a . . . 107(3) ? N2 C3 H3b . . . 109(3) ? C4 C3 H3a . . . 113(4) ? C4 C3 H3b . . . 111(3) ? H3a C3 H3b . . . 107(4) ? N3 C4 C3 . . . 110.4(3) ? N3 C4 H4a . . . 109(4) ? N3 C4 H4b . . . 113(3) ? C3 C4 H4a . . . 111(4) ? C3 C4 H4b . . . 109(3) ? H4a C4 H4b . . . 104(5) ? N3 C5 C6 . . . 111.2(3) ? N3 C5 H5a . . . 111(3) ? N3 C5 H5b . . . 109(3) ? C6 C5 H5a . . . 110(3) ? C6 C5 H5b . . . 110(3) ? H5a C5 H5b . . . 106(4) ? N1 C6 C5 . . . 110.8(3) ? N1 C6 H6a . . . 114(3) ? N1 C6 H6b . . . 110(3) ? C5 C6 H6a . . . 108(3) ? C5 C6 H6b . . . 109(3) ? H6a C6 H6b . . . 105(4) ? O1 C7 O2 . . . 124.7(3) ? O1 C7 C8 . . . 115.3(2) ? O2 C7 C8 . . . 119.9(2) ? N4 C8 C7 . . . 109.5(2) ? N4 C8 C9 . . . 113.2(2) ? N4 C8 H8 . . . 108(3) ? C7 C8 C9 . . . 112.0(2) ? C7 C8 H8 . . . 102(4) ? C9 C8 H8 . . . 111(4) ? C8 C9 C10 . . . 112.5(2) ? C8 C9 H9a . . . 105(3) ? C8 C9 H9b . . . 116(3) ? C10 C9 H9a . . . 113(3) ? C10 C9 H9b . . . 102(4) ? H9a C9 H9b . . . 109(4) ? N5 C10 C9 . . . 120.5(3) ? N5 C10 C11 . . . 106.2(3) ? C9 C10 C11 . . . 133.2(3) ? N6 C11 C10 . . . 107.6(3) ? N6 C11 H11 . . . 126(3) ? C10 C11 H11 . . . 126(3) ? N5 C12 N6 . . . 108.7(3) ? N5 C12 H12 . . . 129(3) ? N6 C12 H12 . . . 122(3) ? F11 P1 F12 . . . 90.93(15) ? F11 P1 F13 . . . 179.02(16) ? F11 P1 F14 . . . 89.64(14) ? F11 P1 F15 . . . 89.81(14) ? F11 P1 F16 . . . 90.87(15) ? F12 P1 F13 . . . 89.94(14) ? F12 P1 F14 . . . 179.08(14) ? F12 P1 F15 . . . 89.73(14) ? F12 P1 F16 . . . 90.69(14) ? F13 P1 F14 . . . 89.49(14) ? F13 P1 F15 . . . 89.73(13) ? F13 P1 F16 . . . 89.58(14) ? F14 P1 F15 . . . 89.56(13) ? F14 P1 F16 . . . 90.02(13) ? F15 P1 F16 . . . 179.20(14) ? Cu F11 P1 . . . 133.53(14) ? F21 P2 F22 . . . 91.00(18) ? F21 P2 F23 . . . 177.73(18) ? F21 P2 F24 . . . 89.92(17) ? F21 P2 F25 . . . 90.89(19) ? F21 P2 F26 . . . 89.24(16) ? F22 P2 F23 . . . 90.45(18) ? F22 P2 F24 . . . 178.02(17) ? F22 P2 F25 . . . 91.5(2) ? F22 P2 F26 . . . 89.22(16) ? F23 P2 F24 . . . 88.58(16) ? F23 P2 F25 . . . 90.8(2) ? F23 P2 F26 . . . 89.02(17) ? F24 P2 F25 . . . 90.22(18) ? F24 P2 F26 . . . 89.04(14) ? F25 P2 F26 . . . 179.2(2) ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 1324 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 15 _reflns_limit_k_min 0 _reflns_limit_k_max 23 _reflns_limit_l_min 0 _reflns_limit_l_max 27 _reflns_number_observed ? _reflns_d_resolution_high .618 _reflns_d_resolution_low 8.583 _diffrn_reflns_av_sigmaI/netI .047 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 153 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .047 _refine_ls_wR_factor_all .056 _refine_ls_goodness_of_fit_all 1.099 _refine_ls_shift/su_mean .001 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_F_squared_meas _refln_F_squared_calc _refln_F_squared_sigma _refln_observed_status _refln_F_meas_friedel _refln_F_sigma_friedel _refln_F_squared_meas_friedel _refln_F_squared_sigma_friedel ? ? ? ? ? ? ? ? ? ? ? ? ? ? #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end